CN114773306A - Method for extracting procyanidine from grape seeds after wine brewing - Google Patents
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- 238000001035 drying Methods 0.000 claims abstract description 11
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- 229920002414 procyanidin Polymers 0.000 description 28
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- MOJZMWJRUKIQGL-FWCKPOPSSA-N Procyanidin C2 Natural products O[C@@H]1[C@@H](c2cc(O)c(O)cc2)Oc2c([C@H]3[C@H](O)[C@@H](c4cc(O)c(O)cc4)Oc4c3c(O)cc(O)c4)c(O)cc(O)c2[C@@H]1c1c(O)cc(O)c2c1O[C@@H]([C@H](O)C2)c1cc(O)c(O)cc1 MOJZMWJRUKIQGL-FWCKPOPSSA-N 0.000 description 20
- HGVVOUNEGQIPMS-UHFFFAOYSA-N procyanidin Chemical compound O1C2=CC(O)=CC(O)=C2C(O)C(O)C1(C=1C=C(O)C(O)=CC=1)OC1CC2=C(O)C=C(O)C=C2OC1C1=CC=C(O)C(O)=C1 HGVVOUNEGQIPMS-UHFFFAOYSA-N 0.000 description 20
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- 239000000178 monomer Substances 0.000 description 3
- GVJHHUAWPYXKBD-UHFFFAOYSA-N (±)-α-Tocopherol Chemical compound OC1=C(C)C(C)=C2OC(CCCC(C)CCCC(C)CCCC(C)C)(C)CCC2=C1C GVJHHUAWPYXKBD-UHFFFAOYSA-N 0.000 description 2
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 2
- NTYJJOPFIAHURM-UHFFFAOYSA-N Histamine Chemical compound NCCC1=CN=CN1 NTYJJOPFIAHURM-UHFFFAOYSA-N 0.000 description 2
- 150000001765 catechin Chemical class 0.000 description 2
- ADRVNXBAWSRFAJ-UHFFFAOYSA-N catechin Natural products OC1Cc2cc(O)cc(O)c2OC1c3ccc(O)c(O)c3 ADRVNXBAWSRFAJ-UHFFFAOYSA-N 0.000 description 2
- 235000005487 catechin Nutrition 0.000 description 2
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- PFTAWBLQPZVEMU-ZFWWWQNUSA-N (+)-epicatechin Natural products C1([C@@H]2OC3=CC(O)=CC(O)=C3C[C@@H]2O)=CC=C(O)C(O)=C1 PFTAWBLQPZVEMU-ZFWWWQNUSA-N 0.000 description 1
- PFTAWBLQPZVEMU-UKRRQHHQSA-N (-)-epicatechin Chemical compound C1([C@H]2OC3=CC(O)=CC(O)=C3C[C@H]2O)=CC=C(O)C(O)=C1 PFTAWBLQPZVEMU-UKRRQHHQSA-N 0.000 description 1
- 102000008186 Collagen Human genes 0.000 description 1
- 108010035532 Collagen Proteins 0.000 description 1
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 description 1
- 206010061218 Inflammation Diseases 0.000 description 1
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- 239000003795 chemical substances by application Substances 0.000 description 1
- 229950001002 cianidanol Drugs 0.000 description 1
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- 238000012364 cultivation method Methods 0.000 description 1
- LPTRNLNOHUVQMS-UHFFFAOYSA-N epicatechin Natural products Cc1cc(O)cc2OC(C(O)Cc12)c1ccc(O)c(O)c1 LPTRNLNOHUVQMS-UHFFFAOYSA-N 0.000 description 1
- 235000012734 epicatechin Nutrition 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- LNTHITQWFMADLM-UHFFFAOYSA-N gallic acid Chemical compound OC(=O)C1=CC(O)=C(O)C(O)=C1 LNTHITQWFMADLM-UHFFFAOYSA-N 0.000 description 1
- WIGCFUFOHFEKBI-UHFFFAOYSA-N gamma-tocopherol Natural products CC(C)CCCC(C)CCCC(C)CCCC1CCC2C(C)C(O)C(C)C(C)C2O1 WIGCFUFOHFEKBI-UHFFFAOYSA-N 0.000 description 1
- 235000021021 grapes Nutrition 0.000 description 1
- 229960001340 histamine Drugs 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000004054 inflammatory process Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 150000008442 polyphenolic compounds Chemical class 0.000 description 1
- 235000013824 polyphenols Nutrition 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- IKGXIBQEEMLURG-NVPNHPEKSA-N rutin Chemical compound O[C@@H]1[C@H](O)[C@@H](O)[C@H](C)O[C@H]1OC[C@@H]1[C@@H](O)[C@H](O)[C@@H](O)[C@H](OC=2C(C3=C(O)C=C(O)C=C3OC=2C=2C=C(O)C(O)=CC=2)=O)O1 IKGXIBQEEMLURG-NVPNHPEKSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- MWOOGOJBHIARFG-UHFFFAOYSA-N vanillin Chemical compound COC1=CC(C=O)=CC=C1O MWOOGOJBHIARFG-UHFFFAOYSA-N 0.000 description 1
- FGQOOHJZONJGDT-UHFFFAOYSA-N vanillin Natural products COC1=CC(O)=CC(C=O)=C1 FGQOOHJZONJGDT-UHFFFAOYSA-N 0.000 description 1
- 235000012141 vanillin Nutrition 0.000 description 1
- 235000019154 vitamin C Nutrition 0.000 description 1
- 239000011718 vitamin C Substances 0.000 description 1
- 235000019165 vitamin E Nutrition 0.000 description 1
- 229940046009 vitamin E Drugs 0.000 description 1
- 239000011709 vitamin E Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- C07D311/58—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4
- C07D311/60—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2
- C07D311/62—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2 with oxygen atoms directly attached in position 3, e.g. anthocyanidins
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B61/00—Dyes of natural origin prepared from natural sources, e.g. vegetable sources
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0096—Purification; Precipitation; Filtration
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention discloses a method for extracting procyanidine by utilizing grape seeds after brewing, which comprises the following steps: (1) crushing grape seeds after brewing, adding ethanol, mixing, and heating in a constant-temperature water bath to obtain a mixed solution; (2) carrying out ultrasonic cell disruption treatment on the mixed solution to obtain a disrupted solution; (3) and carrying out ultrahigh pressure treatment on the crushed liquid, then filtering to obtain a leaching solution, and then concentrating and drying to obtain a finished product of the procyanidine. According to the method, the grape seeds are crudely extracted through the ethanol, then the mixed solution is subjected to cell disruption extraction, the obtained extracting solution is subjected to ultrahigh pressure treatment, and the extraction rate of the procyanidine is greatly improved through the synergistic effect of three steps of extraction.
Description
Technical Field
The invention relates to the technical field of procyanidine extraction, in particular to a method for extracting procyanidine by utilizing grape seeds after brewing.
Background
The grape resources are rich in China, the cultivation area and the yield are in the fifth place of the world, the grape cultivation method is mainly used for producing grape wine, and grape seed skin residue waste generated by wine brewing enterprises is more. In particular, the grape seeds after brewing contain polyphenols (GPS), mainly catechins and proanthocyanidins. The procyanidin is a bioflavonoid, can effectively remove free radicals in vivo, has the oxidation resistance far higher than that of vitamin C and vitamin E, is quickly absorbed, can better exert the function of collagen, and can moisten skin, maintain beauty and keep young; procyanidins also inhibits histamine production and reduces inflammation. The procyanidine has wide efficacy and economic and medicinal development values. Catechin compounds including catechin, epicatechin and gallate thereof are main monomers in grape seed, and are also constitutional units of oligomeric and polymeric procyanidin.
The procyanidin in grape seeds is usually combined with protein and cellulose in a combined state and is not easy to extract, common methods for extracting procyanidin comprise a water extraction method, an organic solvent-water extraction method and an instrument auxiliary extraction method, the water extraction method has long extraction time and high temperature, procyanidin loss is easy to cause, meanwhile, the polarity of water is high, and dissolved impurities are more. Most organic solvents in the organic solvent-water extraction method have great toxic and side effects and low product extraction rate. The instrument-assisted extraction method is difficult to popularize and use due to expensive equipment. The procyanidin has a complex structure composition, and comprises high polymer procyanidin, oligomer procyanidin and procyanidin monomer. Most of the procyanidins with biological activity are oligomeric procyanidins and procyanidin monomers, and most of the procyanidins extracted by the traditional organic solvent method are oligomeric procyanidins and monomeric procyanidins with biological activity, so that the oligomeric procyanidins and the monomeric procyanidins are high polymeric procyanidins without biological activity, and the utilization rate of the biological activity is greatly influenced. Therefore, a method for extracting procyanidine from grape seeds after wine brewing is needed, which can improve the extraction rate of procyanidine and promote the deep fusion development of the wine industry.
Disclosure of Invention
In view of the prior art, the invention aims to provide a method for extracting procyanidine by utilizing grape seeds after wine brewing. According to the method, the grape seeds are crudely extracted through the ethanol, then the mixed solution is subjected to cell disruption extraction, the obtained extracting solution is subjected to ultrahigh pressure treatment, and the extraction rate of the procyanidine is greatly improved through the synergistic effect of three steps of extraction.
In order to realize the purpose, the invention adopts the following technical scheme:
in a first aspect of the present invention, there is provided a method for extracting procyanidins from vinasse, comprising the steps of:
(1) crushing grape seeds after brewing, mixing the grape seeds with ethanol, and heating in a constant-temperature water bath to obtain a mixed solution;
(2) carrying out ultrasonic cell disruption treatment on the mixed solution to obtain a disrupted solution;
(3) and carrying out ultrahigh pressure treatment on the crushed liquid, then filtering to obtain a leaching solution, and then concentrating and drying to obtain a finished product of the procyanidine.
The fermented grape seeds referred to in the present invention refer to grape seeds separated from the fermentation residue after the grapes are fermented.
Preferably, in the step (1), the mass ratio of the grape seed skin residue to the ethanol is 1: (5-8); the mass concentration of the ethanol is 50-70%.
Preferably, in the step (1), the temperature of the constant-temperature water bath heating is 50 ℃, and the time is 1-3 h.
Preferably, in the step (2), the conditions of the ultrasonic cell disruption treatment are as follows: the cell disruption time is 0.5-1 h, the power is 1200-1800W, and the frequency is 25 KHz.
Preferably, in the step (3), the conditions of the ultrahigh pressure treatment are as follows: the pressure is 300-500 MPa and the time is 200-300 s.
The invention has the beneficial effects that:
according to the method, the grape seeds are crudely extracted by the ethanol, then the mixed solution is subjected to cell disruption extraction, the obtained extracting solution is subjected to ultrahigh pressure treatment, and the extraction rate of the procyanidine is greatly improved through the synergistic effect of three steps of extraction.
Detailed Description
It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the disclosure. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.
As described in the background section, the conventional methods for extracting procyanidin include water extraction, organic solvent-water extraction and instrument-assisted extraction, the water extraction takes a long time and has a high temperature, which easily causes loss of procyanidin, and simultaneously, the polarity of water is high and the amount of dissolved impurities is high. Most organic solvents in the organic solvent-water extraction method have great toxic and side effects and low product extraction rate. The instrument-assisted extraction method is difficult to popularize and use due to expensive equipment.
Based on the above, the invention aims to provide a method for extracting procyanidine by utilizing grape seeds after wine brewing. According to the invention, researches show that the extraction rate of the procyanidin obtained by sequentially performing ethanol extraction, cell disruption and ultrahigh pressure treatment is high, and the content of oligomeric procyanidin in the procyanidin obtained by extraction is obviously improved.
In order to make the technical solutions of the present application more clearly understood by those skilled in the art, the technical solutions of the present application will be described in detail below with reference to specific embodiments.
The test materials used in the examples of the present invention are all conventional in the art and commercially available.
Example 1
(1) Separating and selecting 100g of grape seeds with qualified quality from the grape skin residues after brewing, crushing the grape seeds into 20 meshes, and uniformly mixing the grape seeds with 650g of 60% ethanol. Leaching for 2h in a constant-temperature water bath at 50 ℃ to obtain a crude extract.
(2) Placing the crude extract in an ultrasonic cell disruptor: performing cell disruption for 45min under the ultrasonic power of 1800W and the frequency of 25KHz to obtain a disruption solution.
(3) Placing the crushed liquid in a high pressure resistant PE bag for ultrahigh pressure treatment at 400MPa for 240s, filtering the obtained extract to obtain a leaching solution, then carrying out reduced pressure concentration until no alcohol smell exists, recovering ethanol, and drying to obtain procyanidine.
Example 2
(1) Separating and selecting 100g of grape seeds with qualified quality from the grape skin residues after brewing, crushing the grape seeds into 20 meshes, and uniformly mixing the grape seeds with 500g of 70% ethanol. Leaching for 1h in a constant-temperature water bath at 50 ℃ to obtain a crude extract.
(2) And (3) placing the crude extract in an ultrasonic cell disruption instrument for cell disruption for 45min, wherein the ultrasonic power is 1200W, and the frequency is 25KHz to obtain a disrupted solution.
(3) Placing the crushed liquid in a high pressure resistant PE bag for ultrahigh pressure treatment at 300MPa for 300s, filtering the obtained extract to obtain a leaching solution, performing reduced pressure concentration until no alcohol smell exists, recovering ethanol, and drying to obtain procyanidine.
Example 3
(1) Separating and selecting 100g of grape skin residues after brewing wine, crushing the grape skin residues into 20 meshes, and uniformly mixing the grape skin residues with 800g of 50% ethanol. Leaching for 3h in a thermostatic water bath at 50 ℃ to obtain a crude extract.
(2) And (3) placing the crude extract in an ultrasonic cell disruption instrument for cell disruption for 45min, wherein the ultrasonic power is 1200W, and the frequency is 25KHz to obtain a disrupted solution.
(3) Placing the crushed liquid in a high pressure resistant PE bag for ultrahigh pressure treatment at 500MPa for 200s, filtering the obtained extract to obtain a leaching solution, performing reduced pressure concentration until no alcohol smell exists, recovering ethanol, and drying to obtain procyanidine.
Comparative example 1
100g of the grape seeds after brewing are crushed to 20 meshes and are evenly mixed with 650g of 60 percent ethanol. Leaching for 2h in a thermostatic water bath at 50 ℃ to obtain a crude extract. Concentrating under reduced pressure until no alcohol smell is produced, recovering ethanol, and drying to obtain procyanidine.
Comparative example 2
Crushing 100g of brewed grape seeds into 20 meshes, placing the crushed grape seeds and 650g of distilled water in an ultrasonic cell crusher for cell crushing for 45min, wherein the ultrasonic power is 1200W, and the frequency is 25KHz to obtain a crushed liquid. Concentrating under reduced pressure, and drying to obtain 3.21g procyanidin.
Comparative example 3
Crushing 100g of brewed grape seeds into 20 meshes, putting the crushed grape seeds and 650g of distilled water into a high-pressure-resistant PE bag, and performing ultrahigh-pressure treatment at the pressure of 400MPa for 240 s. Concentrating under reduced pressure, and drying to obtain procyanidin.
Comparative example 4
Pulverizing 100g of brewed grape seed to 20 mesh, placing with 60% ethanol in an ultrasonic cell disruptor for cell disruption for 45min, wherein the ultrasonic power is 1200W, and the frequency is 25KHz to obtain disrupted solution. Concentrating under reduced pressure until no alcohol smell is produced, recovering ethanol, and drying to obtain procyanidine.
Comparative example 5
Pulverizing 100g of brewed grape seed to 20 mesh, mixing with 60% ethanol, placing in a high pressure resistant PE bag, and performing ultra high pressure treatment at 400MPa for 240 s. Concentrating under reduced pressure until no alcohol smell is produced, recovering ethanol, and drying to obtain 4.52g procyanidin.
The contents of procyanidins and oligomeric procyanidins in the final extracts (extracts obtained before vacuum concentration) obtained by the methods of examples 1 to 3 and comparative examples 1 to 5 are shown in table 1.
Wherein the content of procyanidin is measured by vanillin method (see determination of procyanidin content of grape seed, Zhao Ping et al, Hebei chemical, 1 month in 2007, vol.30, No. 1), and the content of oligomeric procyanidin in procyanidin is measured by HPLC high performance liquid chromatography method.
TABLE 1
As can be seen from table 1, the content of procyanidine extracted in examples 1 to 3 is 14% or more, which is much higher than that extracted in comparative examples 1 to 5. And as can be seen from table 1, the grape seeds are sequentially subjected to ethanol extraction, cell disruption and ultrahigh pressure treatment, and the three treatments generate synergistic effect, so that the content of procyanidine can be remarkably improved. In addition, the content of the Oligomeric Proanthocyanidin (OPC) in the proanthocyanidins extracted in the examples 1 to 3 is much higher than that in the oligomeric proanthocyanidins extracted in the comparative examples 1 to 5. Compared with other extraction technologies, the extraction method disclosed by the invention does not need to use an organic solvent with high polarity, takes ethanol as an extracting agent, is easy to recover, greatly shortens the extraction time, is low in extraction cost, and is very suitable for industrial production.
The above description is only a preferred embodiment of the present application and is not intended to limit the present application, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present application shall be included in the protection scope of the present application.
Claims (5)
1. The method for extracting procyanidine from grape seeds after wine brewing is characterized by comprising the following steps:
(1) crushing the grape seeds after brewing, adding ethanol, mixing, and heating in a constant-temperature water bath to obtain a mixed solution;
(2) carrying out ultrasonic cell disruption treatment on the mixed solution to obtain a disrupted solution;
(3) and carrying out ultrahigh pressure treatment on the crushed liquid, then filtering to obtain a leaching solution, and then concentrating and drying to obtain a finished product of the procyanidine.
2. The method according to claim 1, wherein in the step (1), the mass ratio of the grape seed skin residue to the ethanol is 1: (5-8); the mass concentration of the ethanol is 50-70%.
3. The method according to claim 1, wherein in the step (1), the temperature of the thermostatic waterbath heating is 50 ℃ and the time is 1-3 h.
4. The method according to claim 1, wherein in the step (2), the conditions of the ultrasonic cell disruption treatment are as follows: the cell disruption time is 0.5-1 h, the power is 1200-1800W, and the frequency is 25 KHz.
5. The method according to claim 1, wherein in the step (3), the conditions of the ultrahigh pressure treatment are as follows: the pressure is 300-500 MPa and the time is 200-300 s.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20050079431A (en) * | 2004-02-05 | 2005-08-10 | (학)청운학원 (대전보건대학) | Method for separating an oligomeric proanthocyanidins from an extract of wild grape seeds |
| CN113951512A (en) * | 2021-11-11 | 2022-01-21 | 郑州轻工业大学 | Grape seed procyanidin oligomer micro powder and preparation method thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20050079431A (en) * | 2004-02-05 | 2005-08-10 | (학)청운학원 (대전보건대학) | Method for separating an oligomeric proanthocyanidins from an extract of wild grape seeds |
| CN113951512A (en) * | 2021-11-11 | 2022-01-21 | 郑州轻工业大学 | Grape seed procyanidin oligomer micro powder and preparation method thereof |
Non-Patent Citations (2)
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